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Sol–gel transition characterization of thermosensitive hydrogels based on water mobility variation provided by low field NMR

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Abstract

Sol–gel transition properties play a key role in various applications of thermosensitive hydrogels, but conventional methods for studying the sol–gel transition have some limitations. For extensive characterization of the water–polymer interaction and microstructure change during sol–gel transition, we propose a rapid and nondestructive method based on monitoring water mobility through low field NMR (LF-NMR), and this was applied to chitosan/β-glycerophosphate (CS/GP) hydrogels. The spin–spin relaxation time (T 2) that depicted water mobility was measured by LF-NMR within 90 s. The T 2 component corresponding to water protons trapped in polymer networks (T 21 ) was very sensitive to sol–gel transition. A remarkable decrease of T 21 value indicated obvious variations of water mobility when CS/GP was heated, and a turning point was observed on the T 21–time curve. The gel point associated with this turning point could be easily determined by fitting the T 21–time curves to a bilinear regression model, and the results showed good accuracy and repeatability owing to the nondestructive nature of LF-NMR. Variations in water components and microstructure of CS/GP caused by water migration after solidification were also analyzed by monitoring dynamic changes of T 2. This rapid, nondestructive method provides a powerful tool for studying the sol–gel transition of hydrogels.

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Abbreviations

CS:

Chitosan

G′:

Elastic modulus

G″:

Viscous modulus

GP:

β-Glycerophosphate

HE T 2 :

Hahn decay time constant

LF-NMR:

Low field NMR

τ:

Pulse spacing

T 2 :

Spin–spin relaxation time

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Acknowledgements

Financial support from the National High Technology Research and Development Program of China (863 Program, Grant Nos. 2014AA021005 and 2014AA021006), the National Natural Science Foundation of China (Grant Nos. 21376248 and 21506228), the National Key Scientific Instrument and Equipment Development Project (Grant No. 2013YQ14040508), the Doctoral Fund of the Ministry of Education (Grant No. 20120181110036), the National Basic Research Program (Grant No. 2013CB733604), and the Opening Foundation of National Key Laboratory of Biochemical Engineering (Grant No. 2014KF-4) is acknowledged.

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    Authors and Affiliations

    1. Key Laboratory of Drug Targeting and Drug Delivery System, Ministry of Education, West China School of Pharmacy, Sichuan University, Chengdu, 610041, People’s Republic of China

      Yaqiong Li & Rong Yu

    2. National Key Laboratory of Biochemical Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing, 100190, People’s Republic of China

      Xiunan Li, Chao Chen, Dawei Zhao, Zhiguo Su & Guanghui Ma

    3. Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing, 210023, People’s Republic of China

      Zhiguo Su

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    Correspondence to Xiunan Li or Rong Yu.

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    Yaqiong Li and Xiunan Li contributed equally to this work.

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    Li, Y., Li, X., Chen, C. et al. Sol–gel transition characterization of thermosensitive hydrogels based on water mobility variation provided by low field NMR. J Polym Res 24, 25 (2017). https://doi.org/10.1007/s10965-017-1185-8

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